#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/16/2011644.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2011644
loop_
_publ_author_name
'Virovets, Alexander V.'
'Kalinina, Irina V.'
'Fedin, Vladimir P.'
'Fenske, Dieter'
_publ_section_title
;Tetragonal polymorphic modification of
 tetrakis(N,N-diethyldithiocarbamato-S,S')tellurium(IV)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e589
_journal_page_last               e590
_journal_paper_doi               10.1107/S0108270100015389
_journal_volume                  56
_journal_year                    2000
_chemical_formula_structural     'C20 H40 N4 S8 Te'
_chemical_formula_sum            'C20 H40 N4 S8 Te'
_chemical_formula_weight         720.64
_chemical_name_common            none
_chemical_name_systematic
;
 tetracis(diethyldithiocarbamato)tellurium(IV)
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3970(15)
_cell_length_b                   10.3970(15)
_cell_length_c                   29.262(6)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    212(2)
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      11.2
_cell_volume                     3163.2(9)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe, 1998)'
_computing_data_reduction        'X-RED  (Stoe, 1998)'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      212(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .021
_diffrn_reflns_av_sigmaI/netI    .0318
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3161
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  .660
_exptl_absorpt_correction_T_min  .596
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .28
_refine_diff_density_max         .291
_refine_diff_density_min         -.279
_refine_ls_abs_structure_details 'Flack (1983), 1094 Friedel pairs'
_refine_ls_abs_structure_Flack   -.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          .040
_refine_ls_R_factor_gt           .029
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0079P)²+5.2275P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .057
_reflns_number_gt                2527
_reflns_number_total             2791
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0439.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 41n 2abw'
_cod_database_code               2011644
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Te1 .43761(3) .56239(3) .7500 .02151(9) Uani d S 1 . . Te
S11 .42914(12) .39940(10) .82649(4) .0287(3) Uani d . 1 . . S
S12 .66612(11) .53125(12) .79778(4) .0339(3) Uani d . 1 . . S
S21 .19313(11) .46936(11) .76072(4) .0329(3) Uani d . 1 . . S
S22 .27112(11) .65413(13) .68924(4) .0336(3) Uani d . 1 . . S
C1 .5912(4) .4240(4) .83389(13) .0269(10) Uani d . 1 . . C
N1 .6578(4) .3632(4) .86666(13) .0351(10) Uani d . 1 . . N
C11 .5945(6) .2774(5) .89921(17) .0474(15) Uani d . 1 . . C
H11A .6457 .1987 .9021 .047 Uiso calc R 1 . . H
H11B .5101 .2532 .8870 .047 Uiso calc R 1 . . H
C12 .5765(7) .3350(6) .94570(19) .0697(19) Uani d . 1 . . C
H12A .6597 .3468 .9601 .070 Uiso calc R 1 . . H
H12B .5242 .2780 .9642 .070 Uiso calc R 1 . . H
H12C .5338 .4176 .9429 .070 Uiso calc R 1 . . H
C13 .7988(5) .3767(5) .87132(18) .0468(15) Uani d . 1 . . C
H13A .8220 .3683 .9036 .047 Uiso calc R 1 . . H
H13B .8239 .4631 .8613 .047 Uiso calc R 1 . . H
C14 .8729(5) .2793(6) .8442(2) .0552(16) Uani d . 1 . . C
H14A .8476 .1934 .8535 .055 Uiso calc R 1 . . H
H14B .9642 .2908 .8495 .055 Uiso calc R 1 . . H
H14C .8547 .2906 .8119 .055 Uiso calc R 1 . . H
C2 .1502(4) .5677(5) .71586(14) .0277(10) Uani d . 1 . . C
N2 .0285(3) .5801(4) .70322(12) .0330(10) Uani d . 1 . . N
C21 -.0123(5) .6597(5) .66391(16) .0398(13) Uani d . 1 . . C
H21A -.0754 .6119 .6457 .040 Uiso calc R 1 . . H
H21B .0624 .6771 .6444 .040 Uiso calc R 1 . . H
C22 -.0710(7) .7863(6) .67908(19) .0628(16) Uani d . 1 . . C
H22A -.1558 .7708 .6917 .063 Uiso calc R 1 . . H
H22B -.0781 .8436 .6530 .063 Uiso calc R 1 . . H
H22C -.0167 .8254 .7022 .063 Uiso calc R 1 . . H
C23 -.0755(5) .5178(5) .72878(16) .0379(12) Uani d . 1 . . C
H23A -.1541 .5690 .7252 .038 Uiso calc R 1 . . H
H23B -.0531 .5177 .7613 .038 Uiso calc R 1 . . H
C24 -.1032(5) .3820(5) .71424(19) .0484(15) Uani d . 1 . . C
H24A -.1259 .3808 .6821 .048 Uiso calc R 1 . . H
H24B -.1742 .3482 .7321 .048 Uiso calc R 1 . . H
H24C -.0275 .3293 .7191 .048 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S11 Te1 S11 8_666 . 132.28(5) yes
S12 Te1 S11 8_666 8_666 63.58(3) no
S12 Te1 S11 . 8_666 83.60(4) yes
S12 Te1 S11 8_666 . 83.60(4) yes
S12 Te1 S11 . . 63.58(3) yes
S12 Te1 S12 8_666 . 93.10(5) yes
S21 Te1 S11 . 8_666 131.50(3) yes
S21 Te1 S11 8_666 8_666 70.51(3) no
S21 Te1 S11 . . 70.51(3) yes
S21 Te1 S11 8_666 . 131.50(3) yes
S21 Te1 S12 . 8_666 82.16(4) yes
S21 Te1 S12 8_666 8_666 134.09(3) no
S21 Te1 S12 . . 134.09(3) yes
S21 Te1 S12 8_666 . 82.16(4) yes
S21 Te1 S21 . 8_666 132.01(5) yes
S22 Te1 S11 . 8_666 81.30(4) yes
S22 Te1 S11 8_666 8_666 136.80(4) no
S22 Te1 S11 . . 136.80(4) yes
S22 Te1 S11 8_666 . 81.30(4) yes
S22 Te1 S12 . 8_666 92.64(4) yes
S22 Te1 S12 8_666 8_666 159.41(4) no
S22 Te1 S12 . . 159.41(4) yes
S22 Te1 S12 8_666 . 92.64(4) yes
S22 Te1 S21 . . 66.35(4) yes
S22 Te1 S21 8_666 . 79.65(4) yes
S22 Te1 S21 . 8_666 79.65(4) yes
S22 Te1 S21 8_666 8_666 66.35(4) no
S22 Te1 S22 . 8_666 88.86(6) yes
C1 S11 Te1 . . 88.86(15) no
C1 S12 Te1 . . 89.85(14) no
C2 S21 Te1 . . 86.74(15) no
C2 S22 Te1 . . 89.17(15) no
S11 C1 S12 . . 117.5(2) no
N1 C1 S11 . . 121.8(4) no
N1 C1 S12 . . 120.7(4) no
C1 N1 C11 . . 121.4(4) no
C1 N1 C13 . . 122.2(4) no
C11 N1 C13 . . 116.4(4) no
N1 C11 C12 . . 113.8(5) no
N1 C13 C14 . . 113.3(4) no
S21 C2 S22 . . 117.6(2) no
N2 C2 S21 . . 121.2(4) no
N2 C2 S22 . . 121.2(4) no
C2 N2 C21 . . 123.0(4) no
C2 N2 C23 . . 121.3(4) no
C23 N2 C21 . . 115.7(4) no
N2 C21 C22 . . 111.9(4) no
N2 C23 C24 . . 114.3(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Te1 S11 8_666 2.8088(11) no
Te1 S11 . 2.8088(11) yes
Te1 S12 8_666 2.7758(12) no
Te1 S12 . 2.7758(13) yes
Te1 S21 . 2.7377(12) yes
Te1 S21 8_666 2.7377(12) no
Te1 S22 . 2.6584(13) yes
Te1 S22 8_666 2.6584(13) no
S11 C1 . 1.718(4) yes
S12 C1 . 1.723(5) yes
S21 C2 . 1.723(5) yes
S22 C2 . 1.730(5) yes
C1 N1 . 1.341(5) yes
N1 C11 . 1.462(7) yes
N1 C13 . 1.479(6) yes
C11 C12 . 1.498(7) yes
C13 C14 . 1.501(7) yes
C2 N2 . 1.325(5) yes
N2 C21 . 1.479(6) yes
N2 C23 . 1.466(6) yes
C21 C22 . 1.517(8) yes
C23 C24 . 1.503(7) yes
